| 第 36 卷第 4 期 |  | Vol. 36 No. 4 | | 2006 年 8 月 | Aug 2006 |
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所屬欄目：有機合成原料
2,3-二甲氧基-1,3-丁二烯的合成研究 |
| 王升文; 鄧建成; 周廣(湘潭大學(xué)化學(xué)學(xué)院; 湖南湘潭) |
| 摘 要：選用新型催化劑及溶劑體系,通過(guò)相轉移催化法在低溫下合成了2,3-二甲氧基-1,3-丁二烯,采用減壓蒸餾和柱層析的分離方法提高了產(chǎn)品純度,通過(guò)在反應前引入吩噻嗪阻聚劑有效防止了產(chǎn)物聚合。實(shí)驗表明:反應以十六烷基三甲基溴化銨作催化劑,v(2,3-丁二酮)∶v(原甲酸甲酯)=1∶3.5,并且在溶劑CH2Cl2中回流10h時(shí),總收率達到77%。與文獻相比,反應條件更溫和,收率更高。 |
| 關(guān)鍵詞：2; 3-二甲氧基-1; 3-丁二烯; 相轉移催化; 合成 |
| 中圖分類(lèi)號：O621.3 文獻標識碼：A 文章編號：1009-9212(2006)04-0057-03 |
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| Synthesis of 2,3-Dimethoxy-1,3-butadiene |
| WANG Sheng-wen; DENG Jian-cheng; ZHOU Guang （Institute of Chemistry; Xiangtan University; Xiangtan 411105; China） |
| Abstract：2,3-dimethoxy-1,3-butadiene was synthesized under low temperature by phase transfer catalyst using new catalyst and solvent, the purity of product could be increased by combination of vaccum-distillation and column chromatography, polymerization of production could be prevented through the addition of phenothiasin before reaction. The experiment showed that the yield of reaction was the highest when cetrimonium bromide was taken as catalyst,the ratio(v : v) of 2,3-Butanedione and methyl o-formate was 1 : 3.... |
| Key words：2; 3-dimethoxy-1; 3-butadiene; phase transfer catalyst; synthesis |
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收稿日期：2006-06-20
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